WO2013125445A1 - Abrasif, ensemble abrasif et procédé d'abrasion d'un substrat - Google Patents

Abrasif, ensemble abrasif et procédé d'abrasion d'un substrat Download PDF

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Publication number
WO2013125445A1
WO2013125445A1 PCT/JP2013/053558 JP2013053558W WO2013125445A1 WO 2013125445 A1 WO2013125445 A1 WO 2013125445A1 JP 2013053558 W JP2013053558 W JP 2013053558W WO 2013125445 A1 WO2013125445 A1 WO 2013125445A1
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WIPO (PCT)
Prior art keywords
abrasive
polishing
insulating material
mass
less
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PCT/JP2013/053558
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English (en)
Japanese (ja)
Inventor
久貴 南
利明 阿久津
友洋 岩野
耕司 藤崎
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日立化成株式会社
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Application filed by 日立化成株式会社 filed Critical 日立化成株式会社
Priority to US14/379,947 priority Critical patent/US9346977B2/en
Priority to KR1020147024909A priority patent/KR102004570B1/ko
Priority to JP2014500685A priority patent/JP6044629B2/ja
Publication of WO2013125445A1 publication Critical patent/WO2013125445A1/fr
Priority to US14/918,834 priority patent/US10196542B2/en

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1409—Abrasive particles per se
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1436—Composite particles, e.g. coated particles
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463—Aqueous liquid suspensions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3105—After-treatment
    • H01L21/31051—Planarisation of the insulating layers
    • H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/76—Making of isolation regions between components
    • H01L21/762—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers
    • H01L21/76224—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers using trench refilling with dielectric materials

Definitions

  • the present invention relates to an abrasive, an abrasive set, and a method for polishing a substrate using the abrasive or the abrasive set.
  • the present invention relates to an abrasive used in a planarization process of a substrate surface, a polishing agent set, and a polishing method for a substrate using the polishing agent or the polishing agent set, which is a manufacturing technique of a semiconductor element.
  • the present invention relates to a polishing agent and a polishing agent set used in a planarization process of a shallow trench isolation (shallow trench isolation, hereinafter referred to as “STI”) insulating material, premetal insulating material, interlayer insulating material, and the like. Further, the present invention relates to a method for polishing a substrate using the abrasive or the abrasive set.
  • STI shallow trench isolation
  • CMP Chemical Mechanical Polishing
  • CMP abrasive The most frequently used CMP abrasive is a silica-based CMP abrasive containing silica (silicon oxide) particles such as fumed silica and colloidal silica as abrasive grains.
  • silica silica
  • silica silica particles
  • fumed silica fumed silica
  • colloidal silica as abrasive grains.
  • Silica-based CMP abrasives are characterized by high versatility, and polishing a wide variety of materials regardless of insulating materials or conductive materials by appropriately selecting the abrasive content, pH, additives, etc. Can do.
  • CMP abrasives containing cerium compound particles as abrasive grains mainly for insulating materials such as silicon oxide is also expanding.
  • a cerium oxide-based CMP abrasive containing cerium oxide (ceria) particles as abrasive grains can polish silicon oxide at high speed even with a lower abrasive grain content than silica-based CMP abrasives (for example, Patent Documents 1 and 2 below) reference).
  • JP-A-10-106994 Japanese Patent Application Laid-Open No. 08-022970 JP 2009-212378 A International Publication No. 2002/067309 JP 2006-249129 A
  • an insulating material such as silicon oxide is polished using silicon nitride, polysilicon or the like as a stopper material (a constituent material of the polishing stopper layer).
  • the polishing selectivity of the insulating material with respect to the stopper material polishing speed ratio: polishing speed of the insulating material / stopper
  • An abrasive having a high material polishing rate is required.
  • the present invention is intended to solve such a technical problem, and can improve the polishing rate of the insulating material, and can improve the polishing selectivity of the insulating material with respect to the stopper material,
  • An object is to provide an abrasive set and a polishing method.
  • the inventors of the present invention studied to increase the interaction between the abrasive grains and the insulating material, and bridged the abrasive grains and the insulating material by hydrogen bonds with a specific glycerin compound. Inventing this, the present invention has been completed.
  • polishing agent of 1st embodiment of this invention contains water, the abrasive grain containing the hydroxide of a tetravalent metal element, and a glycerol compound, and a glycerol compound is represented with the following general formula (I). And at least one selected from the group consisting of compounds represented by the following general formula (II).
  • m is an integer of 3 or more.
  • n represents an integer of 2 or more, and R 1 , R 2 and a plurality of R 3 are each independently a hydrogen atom, a group represented by the following general formula (III), or the following general formula ( And IV).
  • the polishing rate of the insulating material can be improved and the polishing selectivity of the insulating material with respect to the stopper material can be improved as compared with the conventional abrasive. it can.
  • these insulating materials can be polished at high speed in the CMP technique for planarizing the STI insulating material, the premetal insulating material, the interlayer insulating material, and the like.
  • the polishing selectivity of the insulating material with respect to the stopper material can be improved.
  • polishing agent of the 2nd embodiment of this invention contains water, the abrasive grain containing the hydroxide of a tetravalent metal element, and a glycerol compound, and a glycerol compound is polyglycerol, a diglycerol derivative, and poly It is at least one selected from the group consisting of glycerin derivatives, and the glycerin compound has an HLB (Hydrophile-Lipophile Banlance) value of 19.8 to 20.0.
  • HLB Hydrophile Banlance
  • polyglycerin is polyglycerin (polyglycerin of trimer or higher) having an average degree of polymerization of glycerin of 3 or more.
  • diglycerin derivative is a compound in which a functional group is introduced into diglycerin, and “polyglycerin derivative” introduces a functional group into polyglycerol having an average degree of polymerization of glycerin of 3 or more. It is a compound.
  • the polishing rate of the insulating material can be improved and the polishing selectivity of the insulating material with respect to the stopper material can be improved as compared with the conventional abrasive. it can.
  • these insulating materials can be polished at high speed in the CMP technique for planarizing the STI insulating material, the premetal insulating material, the interlayer insulating material, and the like.
  • the polishing selectivity of the insulating material with respect to the stopper material can be improved.
  • an insulating material can also be grind
  • the glycerin compound may be polyoxyalkylene diglyceryl ether or polyoxyalkylene polyglyceryl ether.
  • the hydroxide of the tetravalent metal element is preferably at least one selected from the group consisting of a hydroxide of a rare earth metal element and a hydroxide of zirconium.
  • the average particle size of the abrasive grains is preferably 1 nm or more and 300 nm or less.
  • the content of abrasive grains is preferably 0.005% by mass or more and 20% by mass or less based on the total mass of the abrasive.
  • the weight average molecular weight of the glycerin compound is preferably 250 or more and 10 ⁇ 10 3 or less. Thereby, the polishing rate of the insulating material can be further improved, and the polishing selectivity of the insulating material with respect to the stopper material can be further improved.
  • the content of the glycerin compound is preferably 0.01% by mass or more and 10% by mass or less based on the total mass of the abrasive.
  • the pH of the abrasive according to the present invention is preferably 3.0 or more and 12.0 or less. Thereby, the polishing rate of the insulating material can be further improved, and the polishing selectivity of the insulating material with respect to the stopper material can be further improved.
  • one embodiment of the present invention relates to the use of the abrasive in a polishing method for polishing a surface to be polished containing silicon oxide. That is, the abrasive according to the present invention is preferably used for polishing a surface to be polished containing silicon oxide.
  • the constituents of the abrasive are stored separately in a first liquid and a second liquid, the first liquid contains abrasive grains and water, and the second liquid is glycerin. Contains compound and water.
  • the polishing rate of the insulating material can be improved and the polishing selectivity of the insulating material with respect to the stopper material can be improved as compared with the case where the conventional abrasive is used. .
  • the substrate polishing method of the first embodiment of the present invention may comprise a step of polishing a surface to be polished of the substrate using the abrasive, and the first liquid and the second liquid in the abrasive set.
  • You may provide the process of grind
  • polishing methods by using the polishing agent or the polishing agent set, the polishing rate of the insulating material can be improved as compared with the case of using the conventional polishing agent, and the insulating material with respect to the stopper material can be improved. Polishing selectivity can be improved.
  • the substrate polishing method according to the second embodiment of the present invention is a method for polishing a substrate having an insulating material and polysilicon, wherein the insulating material is selectively polished with respect to polysilicon using the abrasive.
  • polishing selectivity can be improved.
  • the present invention it is possible to provide a polishing agent, a polishing agent set and a polishing method that can improve the polishing rate of the insulating material and improve the polishing selectivity of the insulating material with respect to the stopper material.
  • the polishing agent, the polishing agent set, and the polishing material capable of improving the polishing speed of the insulating material and improving the polishing selectivity of the insulating material with respect to the stopper material, and A polishing method can be provided.
  • these insulating materials can be polished at high speed, and the polishing selectivity of the insulating material with respect to the stopper material can be increased.
  • polishing method can be provided.
  • the insulating material can be polished with low polishing scratches while improving the polishing rate of the insulating material.
  • the abrasive according to this embodiment is a composition that touches the surface to be polished during polishing, and is, for example, a CMP abrasive.
  • polishing agent which concerns on this embodiment contains water, the abrasive grain containing the hydroxide of a tetravalent metal element, and a specific glycerol compound at least.
  • essential components and components that can be optionally added will be described.
  • the abrasive grains are characterized by containing a hydroxide of a tetravalent metal element.
  • the “tetravalent metal element hydroxide” is a compound including a tetravalent metal (M 4+ ) and at least one hydroxide ion (OH ⁇ ) in the present specification.
  • the hydroxide of the tetravalent metal element may contain anions other than hydroxide ions (for example, nitrate ions NO 3 ⁇ and sulfate ions SO 4 2 ⁇ ).
  • a hydroxide of a tetravalent metal element may contain an anion (for example, nitrate ion NO 3 ⁇ , sulfate ion SO 4 2 ⁇ ) bonded to the tetravalent metal element.
  • an anion for example, nitrate ion NO 3 ⁇ , sulfate ion SO 4 2 ⁇
  • Abrasive grains containing tetravalent metal element hydroxide are more reactive with insulating materials (eg, silicon oxide) than conventional abrasive grains made of silica, ceria, etc. Can be polished.
  • insulating materials eg, silicon oxide
  • polishing agent which concerns on this embodiment, in addition to the abrasive grain containing the hydroxide of a tetravalent metal element, you may use another abrasive grain together. Examples of such other abrasive grains include particles of silica, alumina, ceria, and the like.
  • composite particles containing a tetravalent metal element hydroxide and silica can be used as the abrasive grains containing a tetravalent metal element hydroxide and silica can be used.
  • the content of the tetravalent metal element hydroxide is preferably 80% by mass or more, more preferably 90% by mass or more, still more preferably 95% by mass or more, and 98% by mass or more based on the whole abrasive grain. Is particularly preferable, and 99% by mass or more is extremely preferable.
  • the abrasive grains are composed of hydroxides of tetravalent metal elements (100% by mass of the abrasive grains are hydroxide particles of tetravalent metal elements). Most preferred).
  • the tetravalent metal element hydroxide is preferably at least one selected from the group consisting of rare earth metal hydroxides and zirconium hydroxides.
  • a rare earth metal element hydroxide is preferable from the viewpoint of further improving the polishing rate of the insulating material.
  • the rare earth metal element capable of taking tetravalence include lanthanoids such as cerium, praseodymium, and terbium. Among them, lanthanoids are preferable and cerium is more preferable in terms of further improving the polishing rate of the insulating material.
  • a rare earth metal hydroxide and a zirconium hydroxide may be used in combination, or two or more rare earth metal hydroxides may be selected and used.
  • the lower limit of the abrasive or the average particle size of the abrasive grains in the slurry in the abrasive set described later is preferably 1 nm or more, more preferably 2 nm or more, and 3 nm or more. Further preferred.
  • the upper limit of the average particle size of the abrasive grains is preferably 300 nm or less, more preferably 250 nm or less, further preferably 200 nm or less, particularly preferably 100 nm or less, and particularly preferably 50 nm or less, from the viewpoint of further suppressing the surface to be polished from being scratched. Is very preferred.
  • the average grain size of the abrasive grains is more preferably 1 nm or more and 300 nm or less.
  • the “average particle diameter” of the abrasive grains means the average secondary particle diameter of the abrasive grains.
  • the average particle size of the abrasive grains is, for example, a light diffraction scattering type particle size distribution meter (for example, manufactured by Beckman Coulter, Inc., trade name: N5 or manufactured by Malvern Instruments Co., Ltd.) for a slurry in a polishing agent or a polishing agent set described later. , Trade name: Zetasizer 3000HSA).
  • the hydroxide of the tetravalent metal element has a great influence on the polishing characteristics. Therefore, by adjusting the content of the hydroxide of the tetravalent metal element, the chemical interaction between the abrasive grains and the surface to be polished can be improved, and the polishing rate can be further improved. From this, the content of the hydroxide of the tetravalent metal element is preferably 0.01% by mass or more, more preferably 0.03% by mass or more, and more preferably 0.05% by mass or more based on the total mass of the abrasive. preferable.
  • the hydroxide content of the tetravalent metal element makes it easy to avoid agglomeration of the abrasive grains and improves the chemical interaction with the surface to be polished, effectively utilizing the characteristics of the abrasive grains. From the standpoint of possible, it is preferably 8% by mass or less, more preferably 5% by mass or less, still more preferably 3% by mass or less, particularly preferably 1% by mass or less, and particularly preferably 0.5% by mass or less. 0.3 mass% or less is very preferable.
  • the lower limit of the abrasive content is preferably 0.005% by mass or more, more preferably 0.01% by mass or more, based on the total mass of the abrasive, from the viewpoint of further improving the polishing rate of the insulating material.
  • 02 mass% or more is still more preferable, 0.04 mass% or more is especially preferable, and 0.05 mass% or more is very preferable.
  • the upper limit of the abrasive content is preferably 20% by mass or less, more preferably 15% by mass or less, and even more preferably 10% by mass or less, based on the total mass of the abrasive, from the viewpoint of increasing the storage stability of the abrasive. preferable.
  • the content of the abrasive grains is more preferably 0.005% by mass or more and 20% by mass or less based on the total mass of the abrasive.
  • the cost and polishing scratches can be further reduced by further reducing the content of abrasive grains.
  • the content of abrasive grains decreases, the polishing rate of insulating materials and the like also tends to decrease.
  • abrasive grains containing a hydroxide of a tetravalent metal element can obtain a predetermined polishing rate even with a small amount, so that the balance between the polishing rate and the advantage of reducing the content of abrasive grains is balanced. Further, the content of abrasive grains can be further reduced.
  • the content of the abrasive grains is preferably 5% by mass or less, more preferably 3% by mass or less, still more preferably 1% by mass or less, particularly preferably 0.5% by mass or less, and 0.3% by mass. % Or less is very preferable.
  • the abrasive preferably contains a hydroxide of a tetravalent metal element and satisfies at least one of the following conditions (a) and (b).
  • the “aqueous dispersion” in which the content of abrasive grains is adjusted to a predetermined amount means a liquid containing a predetermined amount of abrasive grains and water.
  • Abrasive grains give an absorbance of 1.00 or more to light having a wavelength of 400 nm in an aqueous dispersion in which the content of the abrasive grains is adjusted to 1.0 mass%.
  • the abrasive gives an absorbance of 1.000 or more to light having a wavelength of 290 nm in an aqueous dispersion in which the content of the abrasive is adjusted to 0.0065% by mass.
  • the polishing rate is further improved by using abrasive grains that give an absorbance of 1.00 or more with respect to light having a wavelength of 400 nm in an aqueous dispersion in which the content of abrasive grains is adjusted to 1.0 mass%. be able to. Although this reason is not necessarily clear, this inventor thinks as follows.
  • the tetravalent metal (M 4+ ), 1 to 3 hydroxide ions (OH ⁇ ), and 1 to 3 anions (X c- ) containing M (OH) a X b (wherein a + b ⁇ c 4) is considered to be produced as part of the abrasive grains.
  • the electron-withdrawing anion (X c ⁇ ) acts to improve the reactivity of hydroxide ions, and the amount of M (OH) a X b increases.
  • polishing rate is improved along with this.
  • grains containing M (OH) a Xb absorb the light of wavelength 400nm, since the abundance of M (OH) a Xb increases and the light absorbency with respect to the light of wavelength 400nm becomes high, polishing rate Is thought to improve.
  • abrasive grains containing a tetravalent metal element hydroxide may contain not only M (OH) a Xb but also M (OH) 4 , MO 2 and the like.
  • examples of the anion (X c ⁇ ) include NO 3 ⁇ and SO 4 2 ⁇ .
  • the abrasive grains containing tetravalent metal element hydroxides contain M (OH) a Xb after the abrasive grains are thoroughly washed with pure water and then subjected to the FT-IR ATR (Fourier transform Infrared Spectrometer Attenuated Total).
  • FT-IR ATR Fullier transform Infrared Spectrometer Attenuated Total
  • This can be confirmed by a method of detecting a peak corresponding to an anion (X c ⁇ ) by a reflection method or a Fourier transform infrared spectrophotometer total reflection measurement method.
  • the presence of anions (X c ⁇ ) can also be confirmed by XPS (X-ray Photoelectron Spectroscopy, X-ray photoelectron spectroscopy).
  • the absorption peak at a wavelength of 400 nm of M (OH) a X b (for example, M (OH) 3 X) is much smaller than the absorption peak at a wavelength of 290 nm described later.
  • the present inventor examined the magnitude of the absorbance using an aqueous dispersion having an abrasive content of 1.0% by mass, which has a relatively large abrasive content and is easily detected with a large absorbance. It has been found that when an abrasive that gives an absorbance of 1.00 or more with respect to light having a wavelength of 400 nm is used in an aqueous dispersion, the effect of improving the polishing rate is excellent.
  • the light absorbency with respect to the light of wavelength 400nm originates in an abrasive grain as above-mentioned, it replaces with the abrasive grain which gives the light absorbency 1.00 or more with respect to the light of wavelength 400nm, and with respect to the light of wavelength 400nm.
  • polishing agent containing the substance (for example, pigment component which exhibits yellow) which gives the light absorbency of 1.00 or more it is difficult to obtain the said improvement effect of polishing rate.
  • the polishing rate is further improved by using abrasive grains that give an absorbance of 1.000 or more with respect to light having a wavelength of 290 nm in an aqueous dispersion in which the content of abrasive grains is adjusted to 0.0065% by mass. be able to.
  • a particle containing M (OH) a X b (for example, M (OH) 3 X) generated according to the production conditions of a tetravalent metal element hydroxide has an absorption peak near the wavelength of 290 nm.
  • particles made of Ce 4+ (OH ⁇ ) 3 NO 3 ⁇ have an absorption peak at a wavelength of 290 nm. Therefore, it is considered that the polishing rate is improved as the abundance of M (OH) a Xb increases and the absorbance to light having a wavelength of 290 nm increases.
  • the absorbance with respect to light having a wavelength near 290 nm tends to be detected as it exceeds the measurement limit.
  • the present inventors examined the magnitude of absorbance using an aqueous dispersion having an abrasive content of 0.0065% by mass with a relatively small abrasive content and a low absorbance that is easily detected. It has been found that when an abrasive that gives an absorbance of 1.000 or more with respect to light having a wavelength of 290 nm is used in the aqueous dispersion, the effect of improving the polishing rate is excellent.
  • the present inventor has found that the higher the absorbance of abrasive grains with respect to light near a wavelength of 290 nm, the higher the absorbance of the abrasive grains is, apart from light near a wavelength of 400 nm, where the light-absorbing material tends to exhibit a yellow color. It has been found that the yellowishness of the abrasive and the slurry using the abrasive grains becomes darker, and the polishing rate is improved as the yellowishness of the abrasive and the slurry becomes darker.
  • the lower limit of the absorbance with respect to light having a wavelength of 290 nm is preferably 1.000 or more, more preferably 1.050 or more, still more preferably 1.100 or more, and 1.130 from the viewpoint of polishing the insulating material at a further excellent polishing rate.
  • the above is particularly preferable, and 1.150 or more is very preferable.
  • the upper limit of absorbance for light having a wavelength of 290 nm is not particularly limited, but is preferably 10.00, for example.
  • hydroxides of tetravalent metal elements tend not to absorb light with a wavelength of 450 nm or more, particularly 450 to 600 nm. Therefore, from the viewpoint of polishing the insulating material at an excellent polishing rate by suppressing the adverse effect on polishing due to the inclusion of impurities, the abrasive grains have a content of 0.0065% by mass ( In an aqueous dispersion adjusted to 65 ppm, an absorbance of 0.010 or less is preferably given to light having a wavelength of 450 to 600 nm.
  • the absorbance with respect to all light in the wavelength range of 450 to 600 nm does not exceed 0.010 in the aqueous dispersion in which the content of the abrasive grains is adjusted to 0.0065% by mass.
  • the upper limit of the absorbance with respect to light having a wavelength of 450 to 600 nm is more preferably 0.005 or less, and further preferably 0.001 or less.
  • the lower limit of the absorbance with respect to light having a wavelength of 450 to 600 nm is preferably 0.
  • the absorbance in the aqueous dispersion can be measured using, for example, a spectrophotometer (device name: U3310) manufactured by Hitachi, Ltd. Specifically, for example, an aqueous dispersion in which the content of abrasive grains is adjusted to 1.0 mass% or 0.0065 mass% is prepared as a measurement sample. About 4 mL of this measurement sample is put into a 1 cm square cell, and the cell is set in the apparatus. Next, the absorbance is measured in the wavelength range of 200 to 600 nm, and the absorbance is judged from the obtained chart.
  • a spectrophotometer device name: U3310
  • the absorbance is 1.00 or more when the absorbance for light with a wavelength of 400 nm is measured after being diluted excessively so that the content of the abrasive is less than 1.0% by mass, the content of the abrasive is The absorbance may be screened on the assumption that the absorbance is 1.00 or more even when the content is 1.0 mass%. If the absorbance is 1.000 or more when the absorbance for light having a wavelength of 290 nm is measured after being diluted excessively so that the content of the abrasive is less than 0.0065% by mass, the content of the abrasive is Even when the amount is 0.0065% by mass, the absorbance may be screened on the assumption that the absorbance is 1.000 or more.
  • the absorbance is 0.010 or less when the absorbance with respect to light having a wavelength of 450 to 600 nm is measured by diluting so that the abrasive content is more than 0.0065% by mass, Even when the amount is 0.0065% by mass, the absorbance may be screened on the assumption that the absorbance is 0.010 or less.
  • polishing agent which concerns on this embodiment has high transparency with respect to visible light (it is transparent or close to transparency visually).
  • the abrasive contained in the abrasive according to the present embodiment has a light transmittance of 50% with respect to light having a wavelength of 500 nm in an aqueous dispersion in which the content of the abrasive is adjusted to 1.0 mass%. / Cm or more is preferable. Thereby, since the fall of the grinding
  • the lower limit of the light transmittance is more preferably 60% / cm or more, further preferably 70% / cm or more, particularly preferably 80% / cm or more, extremely preferably 90% / cm or more, 92% / Cm or more is very preferable.
  • the upper limit of the light transmittance is 100% / cm.
  • the abrasive grains present in the aqueous dispersion are particles having a large particle diameter (hereinafter referred to as “coarse particles”). It is considered that there are relatively many.
  • an additive for example, polyvinyl alcohol (PVA)
  • PVA polyvinyl alcohol
  • the number of abrasive grains acting on the surface to be polished per unit area (the number of effective abrasive grains) is reduced, and the specific surface area of the abrasive grains in contact with the surface to be polished is reduced. Conceivable.
  • the abrasive grains present in the aqueous dispersion are in a state of less “coarse particles”.
  • an additive for example, polyvinyl alcohol
  • the number of abrasive grains (number of effective abrasive grains) acting on the surface to be polished per unit area is maintained, and the specific surface area of the abrasive grains in contact with the surface to be polished is maintained. It is considered to be.
  • the light transmittance is a transmittance for light having a wavelength of 500 nm.
  • the light transmittance can be measured with a spectrophotometer. Specifically, for example, it can be measured with a spectrophotometer U3310 (device name) manufactured by Hitachi, Ltd.
  • an aqueous dispersion in which the content of abrasive grains is adjusted to 1.0% by mass is prepared as a measurement sample. About 4 mL of this measurement sample is put into a 1 cm square cell, and the measurement is performed after setting the cell in the apparatus.
  • the content of the abrasive grains is 50% / cm or more in an aqueous dispersion having a content of greater than 1.0% by mass
  • the light transmittance is also obtained when this is diluted to 1.0% by mass. Is apparently 50% / cm or more. Therefore, the light transmittance can be screened by a simple method by using an aqueous dispersion having an abrasive content greater than 1.0% by mass.
  • the absorbance and light transmittance that the abrasive grains contained in the abrasive give in the aqueous dispersion are obtained by removing the solid components other than abrasive grains and the liquid components other than water, and then removing the aqueous dispersion having a predetermined abrasive grain content. It can be prepared and measured using the aqueous dispersion. Although it depends on the components contained in the abrasive, the solid component or the liquid component is removed by, for example, centrifugation using a centrifuge capable of applying a gravitational acceleration of several thousand G or less, or applying a gravitational acceleration of tens of thousands G or more.
  • a compound having a weight average molecular weight of tens of thousands or more for example, 50,000 or more
  • a chromatography method, a filtration method and the like can be mentioned, and among them, gel permeation chromatography and ultrafiltration are preferable.
  • the abrasive grains contained in the abrasive can be passed through the filter by setting appropriate conditions.
  • examples thereof include a chromatography method, a filtration method, and a distillation method, and gel permeation chromatography, ultrafiltration, and vacuum distillation are preferable.
  • abrasive grains When multiple types of abrasive grains are included, filtration methods, centrifugal separation methods, etc. can be mentioned. In the case of filtration, in the filtrate, in the liquid phase, abrasive grains containing a hydroxide of a tetravalent metal element are included. More included.
  • the abrasive grain components can be fractionated and / or other components can be fractionated under the following conditions.
  • Sample solution 100 ⁇ L of abrasive Detector: UV-VIS detector manufactured by Hitachi, Ltd., trade name “L-4200”, wavelength: 400 nm Integrator: Hitachi, Ltd. GPC integrator, product name “D-2500” Pump: Hitachi, Ltd., trade name “L-7100” Column: Hitachi Chemical Co., Ltd. water-based HPLC packed column, trade name “GL-W550S” Eluent: Deionized water Measurement temperature: 23 ° C Flow rate: 1 mL / min (pressure is about 40-50 kg / cm 2 ) Measurement time: 60 minutes
  • a deaeration device it is preferable to deaerate the eluent using a deaeration device before performing chromatography.
  • the deaerator cannot be used, it is preferable to deaerate the eluent in advance with ultrasonic waves or the like.
  • the abrasive components may not be collected even under the above conditions, but in that case, by optimizing the sample solution amount, column type, eluent type, measurement temperature, flow rate, etc. Can be separated.
  • the distillation time of components contained in the abrasive may be adjusted and separated from the abrasive grains.
  • a hydroxide of a tetravalent metal element can be produced by reacting a salt of a tetravalent metal element (metal salt) with an alkali source (base).
  • the hydroxide of the tetravalent metal element is preferably prepared by mixing a salt of the tetravalent metal element and an alkali solution (for example, an alkaline aqueous solution).
  • an alkali solution for example, an alkaline aqueous solution.
  • a hydroxide of a tetravalent metal element can be obtained by mixing a metal salt solution of a salt of a tetravalent metal element (for example, an aqueous metal salt solution) and an alkali solution.
  • a metal salt solution of a salt of a tetravalent metal element for example, an aqueous metal salt solution
  • an alkali solution for example, an alkali solution
  • the means to stir a liquid mixture is not limited.
  • a method of stirring a mixed solution using a bar-like, plate-like or propeller-like stirrer or a stirring blade that rotates around a rotation axis, a magnetic stirrer that transmits power from the outside of a container, and a rotating magnetic field examples include a method of stirring the mixed solution by rotating a stirrer, a method of stirring the mixed solution with a pump installed outside the tank, and a method of stirring the mixed liquid by pressurizing the outside air and blowing it into the tank vigorously.
  • a salt of a tetravalent metal element a conventionally known salt can be used without particular limitation, and M (NO 3 ) 4 , M (SO 4 ) 2 , M (NH 4 ) 2 (NO 3 ) 6 , M (NH 4). ) 4 (SO 4 ) 4 (M represents a rare earth metal element), Zr (SO 4 ) 2 .4H 2 O, and the like. M is preferably chemically active cerium (Ce).
  • optimization of a method for producing a hydroxide of a tetravalent metal element can be mentioned.
  • Specific examples of the method for changing the absorbance with respect to light having a wavelength of 400 nm and the absorbance with respect to light having a wavelength of 290 nm include selection of an alkali source in an alkali solution, adjustment of a raw material concentration in the metal salt solution and the alkali solution, and metal salt Adjustment of the mixing speed of a solution and an alkali liquid adjustment of the liquid temperature of the liquid mixture obtained by mixing the salt of a tetravalent metal element and an alkali source is mentioned.
  • the method for producing a hydroxide of a tetravalent metal element is made more “gradual”. It is preferable.
  • “slow” means that the increase in pH when the pH of the reaction system increases as the reaction proceeds is moderated (slowed).
  • the method for producing a hydroxide of a tetravalent metal element is more “violently”.
  • violently means that the increase in pH when the pH of the reaction system increases as the reaction progresses is increased (accelerated).
  • a method for controlling absorbance and light transmittance will be described in more detail.
  • alkali source examples include organic bases and inorganic bases.
  • Organic bases include nitrogen-containing organic bases such as guanidine, triethylamine and chitosan; nitrogen-containing heterocyclic organic bases such as pyridine, piperidine, pyrrolidine and imidazole; ammonium carbonate, ammonium hydrogen carbonate, tetramethylammonium hydroxide (TMAH), water
  • TMAH tetramethylammonium hydroxide
  • ammonium salts such as tetraethylammonium oxide, tetramethylammonium chloride, and tetraethylammonium chloride.
  • inorganic bases include inorganic salts of alkali metals such as ammonia, lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, lithium carbonate, sodium carbonate, potassium carbonate, lithium hydrogen carbonate, sodium hydrogen carbonate, and potassium hydrogen carbonate.
  • alkali metals such as ammonia, lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, lithium carbonate, sodium carbonate, potassium carbonate, lithium hydrogen carbonate, sodium hydrogen carbonate, and potassium hydrogen carbonate.
  • An alkali source can be used individually by 1 type or in combination of 2 or more types.
  • the alkali source ammonia and imidazole are preferable, and imidazole is more preferable from the viewpoint of further improving the polishing rate of the insulating material.
  • an alkali source exhibiting weak basicity as the alkali source.
  • nitrogen-containing heterocyclic organic bases are preferable, pyridine, piperidine, pyrrolidine, and imidazole are more preferable, pyridine and imidazole are further preferable, and imidazole is particularly preferable.
  • the absorbance with respect to light having a wavelength of 400 nm, the absorbance with respect to light with a wavelength of 290 nm, and the light transmittance with respect to light with a wavelength of 500 nm can be changed.
  • the absorbance tends to increase by increasing the metal salt concentration of the metal salt solution, and the absorbance tends to increase by decreasing the alkali concentration (base concentration, alkali source concentration) of the alkali solution.
  • the light transmittance tends to increase by increasing the metal salt concentration, and the light transmittance tends to increase by decreasing the alkali concentration.
  • the upper limit of the metal salt concentration in the metal salt solution is preferably 1.000 mol / L or less on the basis of the entire metal salt solution, in that it is easy to achieve both excellent polishing rate and excellent abrasive stability. More preferable is 500 mol / L or less, still more preferable is 0.300 mol / L or less, and particularly preferable is 0.200 mol / L or less.
  • the lower limit of the metal salt concentration can suppress the rapid reaction (can moderate the rise in pH), absorbs light with a wavelength of 400 nm, absorbs light with a wavelength of 290 nm, and transmits light with a wavelength of 500 nm. In terms of increasing the rate, it is preferably 0.010 mol / L or more, more preferably 0.020 mol / L or more, and further preferably 0.030 mol / L or more, based on the entire metal salt solution.
  • the upper limit of the alkali concentration in the alkali solution is preferably 15.0 mol / L or less, more preferably 12.0 mol / L or less, and more preferably 10.0 mol based on the whole alkali solution in terms of suppressing the rapid reaction. / L or less is more preferable.
  • the lower limit of the alkali concentration is not particularly limited, but from the viewpoint of productivity, 0.001 mol / L or more is preferable based on the entire alkali solution.
  • the alkali concentration in the alkali solution is preferably adjusted as appropriate depending on the alkali source selected.
  • the upper limit of the alkali concentration is 0.10 mol / L or less based on the whole of the alkali solution in terms of suppressing a rapid reaction. Is preferable, and 0.05 mol / L or less is more preferable.
  • the lower limit of the alkali concentration is not particularly limited, but is 0.001 mol / L or more based on the total amount of the alkali solution in terms of suppressing the use amount of the solution used for obtaining a predetermined amount of tetravalent metal element hydroxide. preferable.
  • the upper limit of the alkali concentration is 1.0 mol / L or less on the basis of the entire alkali solution in terms of suppressing a rapid reaction. Is preferable, and 0.50 mol / L or less is more preferable.
  • the lower limit of the alkali concentration is not particularly limited, but is 0.01 mol / L or more based on the total amount of the alkali solution in terms of suppressing the amount of the solution used for obtaining a predetermined amount of tetravalent metal element hydroxide. preferable.
  • the upper limit of the alkali concentration is preferably 15.0 mol / L or less on the basis of the entire alkali solution, in order to suppress rapid reaction. 10.0 mol / L or less is more preferable.
  • the lower limit of the alkali concentration is not particularly limited, but is 0.10 mol / L or more based on the total amount of the alkali solution in terms of suppressing the amount of the solution used for obtaining a predetermined amount of the tetravalent metal element hydroxide. preferable.
  • Examples of the alkali source in which the pKa of the conjugate acid of the alkali source is 20 or more include 1,8-diazabicyclo [5.4.0] undec-7-ene (pKa: 25).
  • Examples of the alkali source in which the pKa of the conjugate acid of the alkali source is 12 or more and less than 20 include potassium hydroxide (pKa: 16) and sodium hydroxide (pKa: 13).
  • Examples of the alkali source in which the pKa of the conjugate acid of the alkali source is less than 12 include ammonia (pKa: 9) and imidazole (pKa: 7).
  • the pKa value of the conjugate acid of the alkali source used is not particularly limited as long as the alkali concentration is appropriately adjusted, but the pKa of the conjugate acid of the alkali source is preferably less than 20, preferably less than 12. Is more preferably less than 10, and particularly preferably less than 8.
  • the absorbance with respect to light with a wavelength of 400 nm, the absorbance with respect to light with a wavelength of 290 nm, and the light transmittance with respect to light with a wavelength of 500 nm can be changed.
  • the absorbance and the light transmittance are increased by making the increase in pH gentle (slow). More specifically, the absorbance tends to increase by reducing the mixing speed, and the absorbance tends to decrease by increasing the mixing speed.
  • the light transmittance to become high by making a mixing speed slow, and there exists a tendency for the light transmittance to become low by making a mixing speed fast.
  • the upper limit of the mixing speed is preferably 5.00 ⁇ 10 ⁇ 3 m 3 / min (5 L / min) or less from the viewpoint of further suppressing rapid progress of the reaction and further suppressing local reaction bias. 1.00 ⁇ 10 ⁇ 3 m 3 / min (1 L / min) or less, more preferably 5.00 ⁇ 10 ⁇ 4 m 3 / min (500 mL / min) or less, and 1.00 ⁇ 10 ⁇ 4 m 3 / min (100 mL / min) or less is particularly preferable.
  • the lower limit of the mixing speed is not particularly limited, but is preferably 1.00 ⁇ 10 ⁇ 7 m 3 / min (0.1 mL / min) or more from the viewpoint of productivity.
  • the light transmittance with respect to light having a wavelength of 500 nm can be changed. Specifically, the light transmittance tends to increase by increasing the stirring speed, and the light transmittance tends to decrease by decreasing the stirring speed.
  • the lower limit of the stirring speed can further suppress the deviation of the response in the local, and, from the viewpoint of excellent mixing efficiency, preferably 30min -1 or more, more preferably 50min -1 or more, 80min -1 or more is more preferable.
  • the upper limit of the stirring speed is not particularly limited and needs to be adjusted as appropriate depending on the size and shape of the stirring blade, but is preferably 1000 min ⁇ 1 or less from the viewpoint of suppressing liquid splashing.
  • the absorbance for light with a wavelength of 400 nm, the absorbance for light with a wavelength of 290 nm, and the light transmittance for light with a wavelength of 500 nm are obtained.
  • Abrasive grains that can be changed and can achieve a desired polishing rate and storage stability can be obtained.
  • the absorbance tends to increase by lowering the liquid temperature, and the absorbance tends to decrease by increasing the liquid temperature.
  • the light transmittance tends to increase by lowering the liquid temperature, and the light transmittance tends to decrease by increasing the liquid temperature.
  • the liquid temperature is, for example, the temperature in the liquid mixture that can be read by installing a thermometer in the liquid mixture, and is preferably 0 to 100 ° C.
  • the upper limit of the liquid temperature is preferably 100 ° C. or less, more preferably 60 ° C. or less, still more preferably 55 ° C. or less, particularly preferably 50 ° C. or less, and particularly preferably 45 ° C. or less in that rapid reaction can be suppressed. preferable.
  • the lower limit of the liquid temperature is preferably 0 ° C. or higher, more preferably 10 ° C. or higher, and still more preferably 20 ° C. or higher in that the reaction can be easily advanced.
  • the tetravalent metal element hydroxide synthesized by the above method may contain impurities (for example, metal impurities), but the impurities can be removed by washing.
  • impurities for example, metal impurities
  • a method of repeating solid-liquid separation several times by centrifugation or the like can be used. Further, it can be washed by centrifugation, dialysis, ultrafiltration, removal of ions by an ion exchange resin or the like. By removing impurities, the absorbance with respect to light having a wavelength of 450 to 600 nm can be adjusted.
  • the abrasive grains obtained above are agglomerated, they can be dispersed in water by an appropriate method.
  • a method for dispersing abrasive grains in water which is the main dispersion medium, mechanical dispersion treatment using a homogenizer, an ultrasonic disperser, a wet ball mill, or the like may be used in addition to the dispersion treatment using a stirrer.
  • the dispersion method and the particle size control method for example, the method described in Non-Patent Document 1 can be used.
  • the dispersibility of the abrasive grains can also be improved by performing the above-described cleaning treatment to lower the electrical conductivity of the dispersion liquid containing abrasive grains (for example, 500 mS / m or less). Therefore, the cleaning process may be applied as a dispersion process, and the cleaning process and the dispersion process may be used in combination.
  • polishing agent which concerns on this embodiment contains an additive.
  • the “additive” refers to a polishing agent other than water and abrasive grains in order to adjust polishing characteristics such as polishing rate and polishing selectivity; abrasive characteristics such as abrasive dispersibility and storage stability. Refers to the substance added to
  • polishing agent which concerns on this embodiment contains a glycerol compound as a 1st additive.
  • the first additive has an effect of improving the polishing rate of the insulating material. It is considered that the interaction between the abrasive grains and the insulating material can be increased by the interaction between the hydroxyl groups of the glycerin compound and the abrasive grains and the insulating material, and the abrasive grains and the insulating material being bridged by hydrogen bonds.
  • the first additive has an effect of suppressing the polishing rate of the stopper material.
  • the interaction between the abrasive grains and the hydrophobic stopper material can be reduced by the interaction of the hydroxyl groups of the glycerin compound with the abrasive grains to increase the hydrophilicity of the abrasive grain surface.
  • the mechanism of action is not limited to this.
  • the first aspect of the glycerin compound is at least one selected from the group consisting of a compound represented by the following general formula (I) and a compound represented by the following general formula (II).
  • m is an integer of 3 or more.
  • n represents an integer of 2 or more, and R 1 , R 2 and a plurality of R 3 are each independently a hydrogen atom, a group represented by the following general formula (III), or the following general formula ( And IV). However, the case where all of R 1 , R 2 and the plurality of R 3 are hydrogen atoms is excluded.
  • [In formula (III), p represents an integer of 1 or more.
  • q represents an integer of 1 or more. ]
  • m is 3 or more from the viewpoint of improving the polishing rate of the insulating material, preferably 4 or more, more preferably 5 or more, and still more preferably 10 or more. From the viewpoint of production, m is preferably 100 or less, more preferably 50 or less, and still more preferably 30 or less.
  • Examples of the structural unit of the [C 3 H 5 (OH) O] moiety in the formula (I) include structural units represented by the following formulas (Va) to (Vc).
  • the compound represented by the formula (I) may be a compound having one of the formulas (Va) to (Vc), or a compound having a plurality of types of the formulas (Va) to (Vc). May be.
  • the arrangement of the structural units is arbitrary.
  • Examples of the compound represented by the formula (I) include a compound represented by the following formula (VIa) and a compound represented by the following formula (VIb).
  • r1 represents an integer of 0 or more, s1 represents an integer of 0 or more, and r1 + s1 is an integer of 3 or more.
  • r2 represents an integer of 0 or more, s2 represents an integer of 0 or more, and r2 + s2 is an integer of 3 or more.
  • N is 2 or more from the viewpoint of improving the polishing rate of the insulating material. From the viewpoint of production, n is preferably 100 or less, more preferably 50 or less, and still more preferably 30 or less.
  • p is preferably 2 or more and more preferably 5 or more from the viewpoint of further improving the polishing rate of the insulating material. From the viewpoint of further improving the polishing rate of the insulating material, p is preferably 200 or less, more preferably 150 or less, still more preferably 100 or less, and particularly preferably 50 or less. In the formula (IV), q is preferably 2 or more and more preferably 5 or more from the viewpoint of further improving the polishing rate of the insulating material. From the viewpoint of further improving the polishing rate of the insulating material, q is preferably 200 or less, more preferably 150 or less, still more preferably 100 or less, and particularly preferably 50 or less.
  • the second embodiment of the glycerol compound is an embodiment in which the glycerol compound is at least one selected from the group consisting of polyglycerol, diglycerol derivatives and polyglycerol derivatives, and the HLB value of the glycerol compound is 19.8 to 20.0. is there.
  • the compound of the 1st aspect of a glycerol compound may also correspond.
  • Polyglycerin is polyglycerin (polyglycerin of trimer or higher) having an average degree of polymerization of glycerin of 3 or more.
  • the lower limit of the average degree of polymerization of polyglycerin is 3 or more from the viewpoint of increasing the polishing rate of the insulating material, preferably 4 or more, more preferably 5 or more, and still more preferably 10 or more.
  • the upper limit of the average degree of polymerization of polyglycerin is not particularly limited, but is preferably 100 or less, more preferably 50 or less, and even more preferably 30 or less from the viewpoint of production. From the above viewpoint, the average degree of polymerization of polyglycerol is more preferably 3 or more and 100 or less.
  • the diglycerin derivative is a compound in which a functional group is introduced into diglycerin.
  • the functional group include a polyoxyalkylene group.
  • the diglycerin derivative include polyoxyalkylene diglyceryl ether.
  • polyoxyalkylene diglyceryl ether polyoxyethylene diglyceryl ether (Sakamoto Yakuhin Kogyo Co., Ltd., SC-E series, etc.), polyoxypropylene diglyceryl ether (Sakamoto Yakuhin Kogyo Co., Ltd., SY-DP series, etc.) Etc.
  • the polyglycerin derivative is a compound in which a functional group is introduced into polyglycerin having an average degree of polymerization of glycerin of 3 or more.
  • the functional group include a polyoxyalkylene group.
  • the polyglycerin derivative include polyoxyalkylene polyglyceryl ether.
  • the polyoxyalkylene polyglyceryl ether include polyoxyethylene polyglyceryl ether and polyoxypropylene polyglyceryl ether.
  • the HLB value of the second embodiment of the glycerin compound is 19.8 or more, and preferably 19.9 or more, from the viewpoint of excellent dispersion stability.
  • the HLB value of the second embodiment of the glycerin compound is 20.0 or less from the viewpoint of excellent polishing selectivity of the insulating material with respect to the stopper material.
  • the HLB value of the second aspect of the glycerin compound is more preferably 20.0 from the viewpoint of further excellent polishing selectivity of the insulating material with respect to the stopper material.
  • HLB value is a value representing the balance between hydrophilicity and lipophilicity of a compound.
  • the HLB value can be determined by calculation even when the type of hydrophobic group, the type of hydrophilic group, the copolymerization ratio, and the like are different in one compound.
  • HLB value 20 ⁇ (total molecular weight of hydrophilic group part) / (total molecular weight)
  • hydrophilic group examples include a hydroxyl group, a glyceryl group, an oxyethylene group, an oxypropylene group, a hydroxypropyl group, a carboxyl group, and a sulfonic acid group.
  • the compound represented by the formula (II) has an R 1 group, an OR 2 group, and an OC 3 H 5 OR 3 group.
  • R 1 , R 2 and R 3 are all hydrophilic groups
  • the OR 2 group and the OC 3 H 5 OR 3 group are hydrophilic group portions. Therefore, the HLB value of the compound represented by the formula (II) is calculated to be about 20.0.
  • the glycerin compound may not be a single molecule but may have a certain molecular weight distribution.
  • the HLB value of the glycerin compound can be obtained by using an average value of measurement values obtained by measurement by the following method.
  • HLB value of glycerine compound contained in the polishing agent centrifugation, chromatography, filtration, after separation of the glycerine compound from abrasive using a distillation method or the like, performs processing such as concentration if necessary, 13 C- It can be determined by identifying the structure of the compound using NMR, 1 H-NMR, GPC, MALDI-MS (Matrix Assisted Laser Desorption / Ionization-Mass Spectrometry) or the like. For example, the ratio of structural units and the like can be determined from the 1 H-NMR spectrum. The ratio of structural units and the terminal structure can also be identified from the MALDI-MS spectrum. Further, the copolymerization form of the structural unit can be analyzed from the 13 C-NMR spectrum.
  • the first additive can be used alone or in combination of two or more for the purpose of adjusting the polishing selectivity of the insulating material with respect to the stopper material, the flatness, the polishing speed of the insulating material, and the like.
  • a plurality of compounds having different degrees of polymerization can be used in combination.
  • the upper limit of the weight average molecular weight of the first additive is not particularly limited, but is preferably 10 ⁇ 10 3 or less, more preferably 5.0 ⁇ 10 3 or less, from the viewpoint of workability and foamability. 0 ⁇ 10 3 or less is more preferable, and 2.0 ⁇ 10 3 or less is particularly preferable.
  • the first additive is a polyglycerin derivative or a diglycerin derivative
  • the weight average molecular weight of the first additive is from the viewpoint of avoiding a decrease in polishing rate due to the molecular weight of the functional group contained in the derivative being too large.
  • 5.0 ⁇ 10 3 or less is more preferable, 3.0 ⁇ 10 3 or less is more preferable, and 2.0 ⁇ 10 3 or less is particularly preferable.
  • the lower limit of the weight average molecular weight of the first additive is preferably 250 or more, more preferably 400 or more, and further preferably 500 or more, from the viewpoint of further improving the polishing rate of the insulating material.
  • the first additive is polyglycerin, it is preferably 250 or more, more preferably 400 or more, still more preferably 500 or more, particularly preferably 750 or more, from the viewpoint of further improving the polishing rate of the insulating material.
  • 0 ⁇ 10 3 or more is very preferable, and 1.2 ⁇ 10 3 or more is very preferable.
  • the weight average molecular weight of the first additive is more preferably 250 or more and 10 ⁇ 10 3 or less.
  • the weight average molecular weight of a 1st additive can be measured on condition of the following by the gel permeation chromatography method (GPC) using the calibration curve of a standard polystyrene, for example.
  • Equipment used Hitachi L-6000 (made by Hitachi, Ltd.) Column: Gel Pack GL-R420 + Gel Pack GL-R430 + Gel Pack GL-R440 [Hitachi Chemical Co., Ltd., trade name, 3 in total]
  • the lower limit of the content of the first additive is preferably 0.01% by mass or more, more preferably 0.04% by mass or more, based on the total mass of the abrasive, from the viewpoint of further improving the polishing rate of the insulating material. 0.1% by mass or more is more preferable, and 0.3% by mass or more is particularly preferable.
  • the upper limit of the content of the first additive is preferably 10% by mass or less, more preferably 5% by mass or less, based on the total mass of the abrasive, from the viewpoint of suppressing the viscosity of the abrasive from becoming excessively high. .
  • the content of the first additive is more preferably 0.01% by mass or more and 10% by mass or less based on the total mass of the abrasive.
  • the sum total of content of each compound satisfy
  • the abrasive according to the present embodiment includes a second additive in addition to the first additive for the purpose of adjusting polishing characteristics such as a polishing rate; abrasive characteristics such as abrasive dispersibility and storage stability. An agent may be further contained.
  • Examples of the second additive include carboxylic acid and amino acid.
  • a 2nd additive can be used individually by 1 type or in combination of 2 or more types.
  • carboxylic acid and amino acid are preferable from the viewpoint of excellent balance between abrasive dispersibility and polishing characteristics.
  • Carboxylic acid has the effect of stabilizing the pH and further improving the polishing rate of the insulating material.
  • the carboxylic acid include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, and lactic acid.
  • Amino acids have the effect of improving the dispersibility of abrasive grains containing a hydroxide of a tetravalent metal element and further improving the polishing rate of the insulating material.
  • Amino acids include arginine, lysine, aspartic acid, glutamic acid, asparagine, glutamine, histidine, proline, tyrosine, tryptophan, serine, threonine, glycine, alanine, ⁇ -alanine, methionine, cysteine, phenylalanine, leucine, valine, isoleucine, etc. Can be mentioned.
  • an amino acid has a carboxyl group, it shall differ from carboxylic acid.
  • the content of the second additive is 0.01 based on the total mass of the abrasive from the viewpoint of obtaining the additive effect while suppressing sedimentation of the abrasive grains.
  • the mass% is preferably 10% by mass or less.
  • the polishing agent according to this embodiment has flatness, in-plane uniformity, polishing selectivity of silicon oxide with respect to silicon nitride (silicon oxide polishing rate / silicon nitride polishing rate), and polishing selectivity of silicon oxide with respect to polysilicon (
  • a water-soluble polymer may be contained for the purpose of adjusting polishing characteristics such as (silicon oxide polishing rate / polysilicon polishing rate).
  • the “water-soluble polymer” is defined as a polymer that dissolves 0.1 g or more in 100 g of water. The first additive is not included in the “water-soluble polymer”.
  • the water-soluble polymer is not particularly limited.
  • Specific examples of water-soluble polymers include polysaccharides such as alginic acid, pectic acid, carboxymethylcellulose, agar, curdlan, dextrin, cyclodextrin, chitosan, chitosan derivatives, pullulan; polyvinyl alcohol, polyvinylpyrrolidone, polyacrolein, etc.
  • Acrylic polymers such as polyacrylamide and polydimethylacrylamide; Amine polymers such as polyallylamine, polyethyleneimine, and polydiallylamine; polyethylene glycol, polyoxypropylene, polyoxyethylene-polyoxypropylene condensate, ethylenediamine poly Examples thereof include oxyethylene-polyoxypropylene block polymers.
  • These water-soluble polymers may be derivatives. Among water-soluble polymers, amine polymers and derivatives thereof are preferable, and polyallylamine and derivatives thereof are more preferable from the viewpoint of further improving the polishing selectivity of the insulating material with respect to the stopper material.
  • a water-soluble polymer can be used individually by 1 type or in combination of 2 or more types.
  • the weight average molecular weight of the water-soluble polymer is preferably 100 or more, more preferably 300 or more, still more preferably 500 or more, and more preferably 1.0 ⁇ 10 3 or more from the viewpoint of further improving the polishing selectivity of the insulating material with respect to the stopper material. Is particularly preferred.
  • the weight average molecular weight of the water-soluble polymer is preferably 300 ⁇ 10 3 or less, more preferably 100 ⁇ 10 3 or less, and further preferably 50 ⁇ 10 3 or less from the viewpoint of further improving the polishing selectivity of the insulating material with respect to the stopper material. 30 ⁇ 10 3 or less is particularly preferable.
  • the weight average molecular weight of the water-soluble polymer is more preferably from 100 to 300 ⁇ 10 3 .
  • the weight average molecular weight of the water-soluble polymer can be measured by the same method as the weight average molecular weight of the first additive.
  • the content of the water-soluble polymer is 0.0001 on the basis of the total mass of the abrasive from the viewpoint of obtaining the effect of adding the water-soluble polymer while suppressing sedimentation of the abrasive grains. % By mass or more is preferable, 0.00015% by mass or more is more preferable, and 0.0002% by mass or more is more preferable.
  • the content of the water-soluble polymer is preferably 5% by mass or less, preferably 3% by mass or less, based on the total mass of the abrasive, from the viewpoint of obtaining the effect of adding the water-soluble polymer while suppressing sedimentation of the abrasive grains. More preferred is 1% by mass or less.
  • the content of the water-soluble polymer is more preferably 0.0001% by mass or more and 5% by mass or less.
  • the lower limit of the pH (25 ° C.) of the abrasive according to this embodiment is preferably 3.0 or more, more preferably 4.0 or more, and further 4.5 or more.
  • 5.0 or more is particularly preferable.
  • the upper limit of the pH is preferably 12.0 or less, more preferably 11.0 or less, still more preferably 10.0 or less, and particularly preferably 9.0 or less, from the viewpoint of further improving the polishing rate of the insulating material. 8.0 or less is very preferable.
  • the pH of the abrasive is more preferably from 3.0 to 12.0.
  • the pH of the polishing agent can be adjusted by an acid component such as an inorganic acid or an organic acid; an alkali component such as ammonia, sodium hydroxide, tetramethylammonium hydroxide (TMAH), or imidazole.
  • a buffer may be added to stabilize the pH.
  • you may add a buffer as a buffer (liquid containing a buffer). Examples of such a buffer include acetate buffer and phthalate buffer.
  • the pH of the abrasive according to this embodiment can be measured with a pH meter (for example, model number PHL-40 manufactured by Electrochemical Instrument Co., Ltd.). Specifically, for example, after calibrating two pH meters using a phthalate pH buffer solution (pH 4.01) and a neutral phosphate pH buffer solution (pH 6.86) as standard buffers, The value is measured after the electrode is placed in an abrasive and stabilized after 2 minutes or more. At this time, the liquid temperature of the standard buffer and the abrasive is both 25 ° C.
  • a pH meter for example, model number PHL-40 manufactured by Electrochemical Instrument Co., Ltd.
  • the abrasive according to the present embodiment may be stored as a one-component abrasive containing at least abrasive grains, a first additive, and water, and a slurry (first liquid) and an additive liquid (second liquid).
  • a slurry first liquid
  • an additive liquid second liquid
  • the slurry includes at least abrasive grains and water, for example.
  • the additive liquid includes, for example, at least a first additive and water.
  • the first additive, the second additive, the water-soluble polymer, and the buffering agent are included in the additive liquid among the slurry and the additive liquid.
  • the constituents of the abrasive may be stored as an abrasive set divided into three or more liquids.
  • the slurry and additive liquid are mixed immediately before or during polishing to produce an abrasive.
  • the one-component abrasive is stored as an abrasive storage solution with a reduced water content, and may be diluted with water during polishing.
  • the multi-liquid type abrasive set may be stored as a slurry storage solution or an additive storage solution with a reduced water content, and may be diluted with water during polishing.
  • a method of supplying the abrasive onto the polishing surface plate a method of feeding and supplying the abrasive directly; a storage solution for abrasive and water are sent through separate pipes, A method in which these are combined, mixed and supplied; a method in which an abrasive stock solution and water are mixed and supplied in advance can be used.
  • the polishing rate can be adjusted by arbitrarily changing the composition of these liquids.
  • methods for supplying the abrasive onto the polishing surface plate include the following methods. For example, the slurry and the additive liquid are sent through separate pipes, and these pipes are combined, mixed and supplied; the slurry storage liquid, the additive liquid storage liquid and water are sent through separate pipes, A method of supplying these by merging and mixing them; a method of supplying a mixture of slurry and additive solution in advance; a method of supplying a mixture of slurry storage solution, storage solution for additive solution and water in advance, etc. Can do.
  • polishing agent set on a polishing surface plate, respectively can also be used.
  • the surface to be polished is polished using an abrasive obtained by mixing the slurry and the additive liquid on the polishing platen.
  • the substrate polishing method according to the present embodiment may include a polishing step of polishing the surface to be polished of the substrate using the one-part polishing agent, and the slurry and additive liquid in the polishing agent set are mixed. You may provide the grinding
  • the one-part abrasive or the slurry and additive liquid in the abrasive set And a polishing step of selectively polishing the insulating material with respect to polysilicon using a polishing agent obtained by mixing the above.
  • the base may have, for example, a member containing an insulating material and a member containing polysilicon.
  • “selectively polishing material A with respect to material B” means that the polishing rate of material A is higher than the polishing rate of material B under the same polishing conditions. More specifically, for example, the material A is polished with a polishing rate ratio of the polishing rate of the material A to the polishing rate of the material B of 10 or more.
  • the abrasive is supplied between the material to be polished and the polishing pad in a state where the material to be polished of the substrate having the material to be polished is pressed against the polishing pad (polishing cloth) of the polishing surface plate.
  • the surface to be polished of the material to be polished is polished by relatively moving the substrate and the polishing surface plate.
  • at least a part of the material to be polished is removed by polishing.
  • Examples of the substrate to be polished include a substrate.
  • a material to be polished is formed on a substrate for manufacturing a semiconductor element (for example, a semiconductor substrate on which an STI pattern, a gate pattern, a wiring pattern, etc. are formed).
  • a substrate is mentioned.
  • materials to be polished include insulating materials such as silicon oxide; stopper materials such as polysilicon and silicon nitride.
  • the material to be polished may be a single material or a plurality of materials. When a plurality of materials are exposed on the surface to be polished, they can be regarded as materials to be polished.
  • the material to be polished may be in the form of a film, and may be a silicon oxide film, a polysilicon film, a silicon nitride film, or the like.
  • the material to be polished (such as an insulating material such as silicon oxide) formed on such a substrate is polished with the above-described abrasive and the excess portion is removed, so that the unevenness of the surface of the material to be polished is eliminated and the material to be polished is removed. It can be a smooth surface over the entire surface of the abrasive material.
  • the abrasive according to this embodiment is preferably used for polishing a surface to be polished containing silicon oxide.
  • the stopper material constituting the stopper is a material whose polishing rate is lower than that of the insulating material, and polysilicon, silicon nitride and the like are preferable.
  • the polishing is stopped when the stopper is exposed, the insulating material can be prevented from being excessively polished, and thus the flatness of the insulating material after polishing can be improved.
  • a low pressure CVD method As a method for producing a material to be polished by the polishing agent according to the present embodiment, a low pressure CVD method, a quasi-atmospheric pressure CVD method, a plasma CVD method or other CVD method; a spin coating method in which a liquid material is applied to a rotating substrate Etc.
  • Silicon oxide can be obtained, for example, by thermally reacting monosilane (SiH 4 ) and oxygen (O 2 ) using a low pressure CVD method. Silicon oxide can be obtained, for example, by thermally reacting tetraethoxysilane (Si (OC 2 H 5 ) 4 ) and ozone (O 3 ) using a quasi-atmospheric pressure CVD method. As another example, silicon oxide is similarly obtained by causing plasma reaction between tetraethoxysilane and oxygen.
  • Silicon oxide is obtained by applying a liquid raw material containing, for example, inorganic polysilazane, inorganic siloxane, etc. on a substrate using a spin coating method, and performing a thermosetting reaction in a furnace body or the like.
  • Examples of the method for producing polysilicon include a low pressure CVD method in which monosilane is thermally reacted, a plasma CVD method in which monosilane is subjected to plasma reaction, and the like.
  • silicon nitride for example, a low pressure CVD method in which dichlorosilane and ammonia are reacted by heat, a plasma CVD method in which monosilane, ammonia and nitrogen are subjected to plasma reaction, and the like can be given.
  • the silicon nitride obtained by the above method may contain elements other than silicon and nitrogen, such as carbon and hydrogen, in order to adjust the material.
  • heat treatment may be performed at a temperature of 200 to 1000 ° C. as necessary.
  • the silicon oxide obtained by the above method may contain a small amount of boron (B), phosphorus (P), carbon (C) or the like in order to improve the embedding property.
  • polishing method for a semiconductor substrate on which an insulating material is formed.
  • a polishing apparatus a general polishing apparatus having a holder capable of holding a substrate such as a semiconductor substrate having a surface to be polished and a polishing surface plate to which a polishing pad can be attached. Can be used.
  • Each of the holder and the polishing surface plate is provided with a motor capable of changing the rotation speed.
  • a polishing apparatus for example, a polishing apparatus: Reflexion manufactured by APPLIED MATERIALS can be used.
  • polishing pad general nonwoven fabric, foam, non-foam, etc.
  • material of the polishing pad include polyurethane, acrylic, polyester, acrylic-ester copolymer, polytetrafluoroethylene, polypropylene, polyethylene, poly-4-methylpentene, cellulose, cellulose ester, polyamide (for example, nylon (trade name) and Aramid), polyimide, polyimide amide, polysiloxane copolymer, oxirane compound, phenol resin, polystyrene, polycarbonate, epoxy resin and the like can be used.
  • the material of the polishing pad in particular, foamed polyurethane and non-foamed polyurethane are preferable from the viewpoint of polishing speed and flatness. It is preferable that the polishing pad is grooved so as to collect the abrasive.
  • the rotation speed of the polishing platen is preferably 200 min ⁇ 1 or less so that the semiconductor substrate does not pop out, and the polishing pressure (processing load) applied to the semiconductor substrate is such that polishing flaws occur. From the viewpoint of sufficiently suppressing, 100 kPa or less is preferable.
  • the surface of a polishing pad is always covered with the abrasive
  • the semiconductor substrate after polishing is preferably washed well under running water to remove particles adhering to the substrate.
  • dilute hydrofluoric acid or ammonia water may be used in addition to pure water, and a brush may be used in combination to increase cleaning efficiency.
  • a spin dryer or the like it is preferable to dry the semiconductor substrate after removing water droplets adhering to the semiconductor substrate using a spin dryer or the like.
  • the abrasive, the abrasive set and the polishing method according to this embodiment can be suitably used for forming STI.
  • the polishing rate ratio of the insulating material (for example, silicon oxide) to the stopper material (for example, polysilicon) is preferably 10 or more, and more preferably 12 or more.
  • the polishing rate ratio is less than 10
  • the polishing rate of the insulating material relative to the polishing rate of the stopper material is small, and it tends to be difficult to stop polishing at a predetermined position when forming the STI.
  • the polishing rate ratio is 10 or more, the polishing can be easily stopped, which is more suitable for the formation of STI.
  • the polishing agent, the polishing agent set and the polishing method according to this embodiment can also be used for polishing a premetal insulating material.
  • a premetal insulating material for example, phosphorus-silicate glass and boron-phosphorus-silicate glass are used in addition to silicon oxide, and silicon oxyfluoride, fluorinated amorphous carbon, and the like can also be used.
  • the abrasive, the abrasive set and the polishing method according to this embodiment can be applied to materials other than insulating materials such as silicon oxide.
  • materials include high dielectric constant materials such as Hf-based, Ti-based, and Ta-based oxides; semiconductor materials such as silicon, amorphous silicon, SiC, SiGe, Ge, GaN, GaP, GaAs, and organic semiconductors; GeSbTe Inorganic conductive materials such as ITO; Polymer resins such as polyimides, polybenzoxazoles, acrylics, epoxies, and phenols.
  • the polishing agent, the polishing agent set, and the polishing method according to the present embodiment are not only film-like objects to be polished, but also various types composed of glass, silicon, SiC, SiGe, Ge, GaN, GaP, GaAs, sapphire, plastic, or the like. It can also be applied to substrates.
  • the polishing agent, the polishing agent set, and the polishing method according to the present embodiment are not only for manufacturing semiconductor elements, but also for image display devices such as TFTs and organic ELs; optical parts such as photomasks, lenses, prisms, optical fibers, and single crystal scintillators Optical elements such as optical switching elements and optical waveguides; light emitting elements such as solid lasers and blue laser LEDs; and magnetic storage devices such as magnetic disks and magnetic heads.
  • the obtained dispersion of cerium hydroxide particles was subjected to solid-liquid separation by centrifugation (4000 min ⁇ 1 , 5 minutes), and a precipitate having a solid content of about 10% was taken out.
  • the precipitate obtained by solid-liquid separation is mixed with water so that the cerium hydroxide content is 1.0% by mass, and the particles are dispersed in water using an ultrasonic cleaning machine.
  • a stock slurry was prepared.
  • the measuring method is as follows. First, about 1 mL of a measurement sample (aqueous dispersion) containing 1.0% by mass of cerium hydroxide particles was placed in a 1 cm square cell, and the cell was placed in N5. The refractive index of the measurement sample was adjusted to 1.333, the viscosity of the measurement sample was adjusted to 0.887 mPa ⁇ s, the measurement was carried out at 25 ° C., and the value displayed as Unimodal Size Mean was read.
  • the abrasive grains contained in the cerium hydroxide slurry stock solution contained at least some particles having nitrate ions bonded to the cerium element.
  • the abrasive grains contained cerium hydroxide because they contained at least part of particles having hydroxide ions bonded to cerium element.
  • a cerium hydroxide slurry storage solution (particle content: 1.0 mass%) is placed in a 1 cm square cell, and the cell is placed in a spectrophotometer (device name: U3310) manufactured by Hitachi, Ltd. did.
  • Absorbance was measured in the wavelength range of 200 to 600 nm, and the absorbance with respect to light with a wavelength of 400 nm and the light transmittance with respect to light with a wavelength of 500 nm were measured.
  • Absorbance with respect to light with a wavelength of 400 nm was 2.25, and light transmittance with respect to light with a wavelength of 500 nm was 92% / cm.
  • CMP abrasives used in Examples 1 to 8 and Comparative Examples 1 to 7 were 0.05% by mass of cerium hydroxide particles as abrasive grains and 0% of the additives shown in Table 1 based on the total mass of the CMP abrasive. It was prepared to contain ⁇ 0.5 mass%, 0.005 mass% imidazole as a pH adjusting agent, and pure water in the balance. After dissolving components other than abrasive grains in pure water, a cerium hydroxide slurry stock solution was mixed and stirred to prepare a CMP abrasive.
  • the additive used in the Examples is a compound having the following structure.
  • SC-E2000 diglycerin polyether (polyoxyethylene diglyceryl ether) manufactured by Sakamoto Yakuhin Kogyo): a compound satisfying formula (II) (R 1 : group represented by formula (III), R 2 : hydrogen atom,
  • PH Measurement temperature: 25 ⁇ 5 ° C
  • Measuring device manufactured by Electrochemical Instrument Co., Ltd., model number PHL-40 Measurement method: After calibrating two points using a standard buffer (phthalate pH buffer, pH: 4.01 (25 ° C.); neutral phosphate pH buffer, pH 6.86 (25 ° C.)), The electrode was placed in a CMP abrasive and the pH after the passage of 2 minutes or more and stabilized was measured with the measuring device.
  • a standard buffer phthalate pH buffer, pH: 4.01 (25 ° C.); neutral phosphate pH buffer, pH 6.86 (25 ° C.)
  • the average particle diameter of the cerium hydroxide particles in the CMP abrasive was measured using a product name: N5 manufactured by Beckman Coulter.
  • the measuring method is as follows. First, about 1 mL of CMP abrasive was placed in a 1 cm square cell, and the cell was placed in N5. The refractive index of the measurement sample was adjusted to 1.333, the viscosity of the measurement sample was adjusted to 0.887 mPa ⁇ s, the measurement was carried out at 25 ° C., and the value displayed as Unimodal Size Mean was read.
  • ⁇ CMP polishing conditions> The substrate to be polished was polished under the following polishing conditions using a CMP abrasive.
  • the substrate having the polysilicon film was polished in Examples 1 to 8 and Comparative Examples 1 and 7. In Comparative Examples 2 to 6, since the polishing rate of the silicon oxide film was low, the substrate having the polysilicon film was not polished.
  • Polishing equipment Reflexion (manufactured by APPLIED MATERIALS) CMP polishing agent flow rate: 200 mL / min
  • CMP polishing agent flow rate 200 mL / min
  • Substrate to be polished a substrate in which a silicon oxide film having a thickness of 1 ⁇ m is formed on a silicon substrate by a plasma CVD method, and a polysilicon film having a thickness of 0.2 ⁇ m on a silicon substrate by a CVD method
  • Polishing pad Foamed polyurethane resin with closed cells (Rohm and Haas Japan, model number IC1000) Polishing pressure: 14.7 kPa (2 psi) Relative speed between substrate and polishing platen: 85 m / min Polishing time: 1 minute
  • Cleaning After CMP treatment, cleaning with ultrasonic water was performed and then drying with a spin dryer.
  • the polishing rate (silicon oxide polishing rate: SiO 2 RR, polysilicon polishing rate: p-SiRR) of the film to be polished (silicon oxide film, polysilicon film) polished and cleaned under the above conditions was determined from the following equation.
  • the film thickness difference of the film to be polished before and after polishing was determined using an optical interference film thickness apparatus (manufactured by Filmetrics, trade name: F80).
  • (Polishing rate: RR) (Thickness difference of the film to be polished before and after polishing (nm)) / (Polishing time (min))
  • the substrate to be polished (blanket wafer substrate having a silicon oxide film) polished and cleaned under the above conditions was immersed in an aqueous solution of 0.5% by mass of hydrogen fluoride for 15 seconds and then washed with water for 60 seconds. Subsequently, the surface of the film to be polished was washed for 1 minute while supplying water using a polyvinyl alcohol brush, and then dried. A defect of 0.2 ⁇ m or more on the surface of the film to be polished was detected using Complied by APPLIED MATERIALS.
  • the number of polishing scratches of 0.2 ⁇ m or more on the surface of the film to be polished was In all of the comparative examples, it was about 0 to 3 (pieces / wafer), and the generation of polishing scratches was sufficiently suppressed.
  • the silicon oxide polishing rate (SiO 2 RR), the polysilicon polishing rate (p-SiRR), the polishing selectivity ratio of the silicon oxide polishing rate / polysilicon polishing rate in Examples 1 to 8 and Comparative Examples 1 to 7 are shown. It is shown in 1.
  • the HLB value of the additives of Examples 1 to 8 was 20.0.
  • the polyglycerin fatty acid ester of Comparative Example 7 (polyglycerin average polymerization degree: 4, HLB value: 12.2) corresponds to the compounds represented by the general formulas (I) and (II) in that it is a fatty acid ester. It is not a compound.
  • Example 1 0.5 mass% of polyglycerin tetramer (weight average molecular weight: 300) was used in the production of the CMP abrasive.
  • the silicon oxide polishing rate was 200 nm / min, which was higher than Comparative Examples 1-7.
  • the polishing selectivity was 11, which was higher than those of Comparative Examples 1 and 7.
  • Example 2 0.5 mass% of polyglycerin hexamer (weight average molecular weight: 420) was used in the production of the CMP abrasive.
  • the silicon oxide polishing rate was 225 nm / min, which was higher than Comparative Examples 1-7. Further, the polishing selectivity was 11, which was higher than those of Comparative Examples 1 and 7.
  • Example 3 0.5% by mass of polyglycerin 10-mer (weight average molecular weight: 680) was used in the production of the CMP abrasive.
  • the silicon oxide polishing rate was 280 nm / min, which was higher than Comparative Examples 1-7.
  • the polishing selectivity was 12, which was higher than Comparative Examples 1 and 7.
  • Example 4 0.5% by mass of polyglycerol 20-mer (weight average molecular weight: 1300) was used in the production of the CMP abrasive.
  • the silicon oxide polishing rate was 315 nm / min, which was higher than Comparative Examples 1-7. Further, the polishing selectivity was 14, which was higher than those of Comparative Examples 1 and 7.
  • Example 5 0.5% by mass of SC-E450 (diglycerin polyether (polyoxyethylene diglyceryl ether), weight average molecular weight: 450) manufactured by Sakamoto Yakuhin Kogyo Co., Ltd. was used in the production of the CMP abrasive.
  • SC-E450 diglycerin polyether (polyoxyethylene diglyceryl ether), weight average molecular weight: 450) manufactured by Sakamoto Yakuhin Kogyo Co., Ltd.
  • the silicon oxide polishing rate was 230 nm / min, which was higher than Comparative Examples 1-7.
  • the polishing selectivity was 14, which was higher than those of Comparative Examples 1 and 7.
  • Example 6 0.5% by mass of SC-E2000 (diglycerin polyether (polyoxyethylene diglyceryl ether), weight average molecular weight: 2000) manufactured by Sakamoto Pharmaceutical Co., Ltd. was used in the production of the CMP abrasive.
  • SC-E2000 diglycerin polyether (polyoxyethylene diglyceryl ether), weight average molecular weight: 2000) manufactured by Sakamoto Pharmaceutical Co., Ltd. was used in the production of the CMP abrasive.
  • the silicon oxide polishing rate was 210 nm / min, which was higher than Comparative Examples 1-7. Further, the polishing selectivity was 14, which was higher than those of Comparative Examples 1 and 7.
  • Example 7 0.5 mass% of SC-E4500 (diglycerin polyether (polyoxyethylene diglyceryl ether), weight average molecular weight: 4500) manufactured by Sakamoto Yakuhin Kogyo Co., Ltd. was used in the production of the CMP abrasive.
  • SC-E4500 diglycerin polyether (polyoxyethylene diglyceryl ether), weight average molecular weight: 4500
  • the silicon oxide polishing rate was 195 nm / min, which was higher than Comparative Examples 1-7.
  • the polishing selectivity was 12, which was higher than Comparative Examples 1 and 7.
  • Example 8 0.05% by mass of polyglycerin 20-mer (weight average molecular weight: 1300) was used in the production of the CMP abrasive.
  • the silicon oxide polishing rate was 270 nm / min, which was higher than Comparative Examples 1-7.
  • the polishing selectivity was 12, which was higher than Comparative Examples 1 and 7.
  • the present invention it is possible to provide a polishing agent, a polishing agent set and a polishing method that can improve the polishing rate of the insulating material and improve the polishing selectivity of the insulating material with respect to the stopper material.
  • the insulating material in particular, in CMP technology for flattening an STI insulating material, a premetal insulating material, an interlayer insulating material, etc., the insulating material can be polished at a high speed and the polishing selectivity of the insulating material with respect to the stopper material is improved.
  • An abrasive, an abrasive set and a polishing method can be provided.
  • the insulating material can be polished with low polishing scratches while improving the polishing rate of the insulating material.

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Abstract

La présente invention concerne un abrasif qui contient : de l'eau ; un grain abrasif contenant l'hydroxyde d'un élément métallique tétravalent ; et un composé de glycérine spécifique.
PCT/JP2013/053558 2012-02-21 2013-02-14 Abrasif, ensemble abrasif et procédé d'abrasion d'un substrat WO2013125445A1 (fr)

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